X-ray spectroscopy is generally accepted as the most useful ancillary technique that can be added to any scanning electron microscope (SEM), even to the point of being considered a necessity by most operators. While “stand-alone” x-ray detection systems are used less frequently in failure analysis than the more exact instrumentation employed in SEMs, the technology is advancing and is worthy of note due to its capability for nondestructive analysis and application in the field. This article begins with information on the basis of the x-ray signal. This is followed by information on the operating principles and applications of detectors for x-ray spectroscopy, namely energy-dispersive spectrometers, wavelength-dispersive spectrometers, and handheld x-ray fluorescence systems. The processes involved in x-ray analysis in the SEM and handheld x-ray fluorescence analysis are then covered. The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis.

This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.

A steel pot used as crucible in a magnesium alloy foundry developed a leak that resulted in a fire and caused extensive damage. Hypotheses as to the cause of the leak included a defect in the pot, overuse, overheating, and poor foundry practices. Scanning electron microscopy, transmission electron microscopy, optical microscopy, and x-ray microanalysis in conjunction with dimensional analysis, phase diagrams and thermodynamics considerations were employed to evaluate the various hypotheses. All evidence pointed to an oxide mass in the area where the hole developed, likely introduced during the steelmaking process.

This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.

Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.

Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.

Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

This article provides information on the chemical characterization of surfaces by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). It describes the basic theory behind each of these techniques, the types of data produced from each, and some typical applications. The article explains the strengths of AES, XPS, and TOF-SIMS based on data obtained from the surface of a slightly corroded stainless steel sheet.

The scanning electron microscopy (SEM) is one of the most versatile instruments for investigating the microstructure of metallic materials. This article highlights the development of SEM technology and describes the operation of basic systems in an SEM, including the electron optical column, signal detection and display equipment, and vacuum system. It discusses the preparation of samples for observation using an SEM and describes the application of SEM in fractography. If the surface remains unaffected and undamaged by events subsequent to the actual failure, it is often a simple matter to determine the failure mode by the use of an SEM. In cases where the surface is altered after the initial failure, the case may not be so straightforward. The article presents typical examples that illustrate these points. Image dependence on the microscope type and operating parameters is also discussed.

A failure analysis was conducted in late 1996 on two rolls that had been used in the production of iron and steel powder. The rolls had elongated over their length such that the roll trunnions had impacted with the furnace wall refractory. The result was distortion and bowing of the roll bodies which necessitated their removal from service. The initial analysis found large quantities of nitrogen had been absorbed by the roll shell. Further research indicated nitrogen pickup accounted for 3% volumetric growth for every 1% by weight nitrogen absorption. This expansion was sufficient to account for the dimensional change observed in the failed rolls. This paper details the failure analysis and resulting research it inspired. It also provides recommendations for cast material choice in highly nitriding atmospheres.

This article outlines the basic steps to be followed and the range of techniques available for failure analysis, namely, background data assembling, visual examination, microfractography, chemical analysis, metallographic examination, electron microscopy, electron microprobe analysis, X-ray techniques, and simulations. It also describes the steps for analyzing the data, preparing the report, preservation of evidence, and follow-up on recommendations.

This article describes the characteristics of tubing of heat exchangers with respect to general corrosion, stress-corrosion cracking, selective leaching, and oxygen-cell attack, with examples. It illustrates the examination of failed parts of heat exchangers by using sample selection, visual examination, microscopic examination, chemical analysis, and mechanical tests. The article explains corrosion fatigue of tubing of heat exchangers caused by aggressive environment and cyclic stress. It also discusses the effects of design, welding practices, and elevated temperatures on the failures of heat exchangers.

This article describes the preliminary stages and general procedures, techniques, and precautions employed in the investigation and analysis of metallurgical failures that occur in service. The most common causes of failure characteristics are described for fracture, corrosion, and wear failures. The article provides information on the synthesis and interpretation of results from the investigation. Finally, it presents key guidelines for conducting a failure analysis.

Stress-corrosion cracking (SCC) is a form of corrosion and produces wastage in that the stress-corrosion cracks penetrate the cross-sectional thickness of a component over time and deteriorate its mechanical strength. Although there are factors common among the different forms of environmentally induced cracking, this article deals only with SCC of metallic components. It begins by presenting terminology and background of SCC. Then, the general characteristics of SCC and the development of conditions for SCC as well as the stages of SCC are covered. The article provides a brief overview of proposed SCC propagation mechanisms. It discusses the processes involved in diagnosing SCC and the prevention and mitigation of SCC. Several engineering alloys are discussed with respect to their susceptibility to SCC. This includes a description of some of the environmental and metallurgical conditions commonly associated with the development of SCC, although not all, and numerous case studies.

Heat exchangers are devices used to transfer thermal energy between two or more fluids, between a solid surface and a fluid, or between a solid particulate and a fluid at different temperatures. This article first addresses the causes of failures in heat exchangers. It then provides a description of heat-transfer surface area, discussing the design of the tubular heat exchanger. Next, the article discusses the processes involved in the examination of failed parts. Finally, it describes the most important types of corrosion, including uniform, galvanic, pitting, stress, and erosion corrosion.